船舶机械油液检测光谱分析的特征参数研究

通过对机械设备润滑油的长期光谱跟踪检测分析,建立基于光谱分析的润滑油状态监测故障诊断数学模型。通过实验研究和机械设备润滑油油样的实际光谱检测分析相结合,根据不同机械设备的磨损特征元素确定机械设备基于油液检测光谱分析故障诊断的特征参数,以确定机械设备发生故障的时间,从而避免重大故障的突发,为机械设备实现视情维修提供理论和实际依据,提高机械设备的可靠性和可维修性。故障诊断实例证明,此特征参数具有较高的稳定性和准确性,能够有效地应用于各种机械设备的油液检测的故障诊断中。     

Detection of hydrogen isotope atoms by mass spectrometry combined with resonant ionization

We examined the application of mass spectrometric methods using resonant ionization by a tunable laser and proposed its use for analyzing hydrogen isotopes. We conducted resonance ionization mass spectrometry (RIMS) to detect gas-phase hydrogen isotope atoms. The ionization efficiency was increased by more than 1000 times that obtained with conventional methods using nonresonant ionization. Resonant laser ablation mass spectrometry (RLAMS) was applied for deuterium detection in solid samples. A graphite substrate implanted with deuterium was used for ordinary laser ablation mass spectrometry (LAMS) and RLAMS. The deuterium signal was observed very clearly by RLAMS, in contrast to LAMS. Mass spectrometry combined with resonance ionization was very useful for hydrogen isotope detection, because components with equal mass numbers were resolved and the method demonstrated higher ionization efficiency. Received: 4 November 1998 / Revised version: 12 January 1999 / Published online: 7 April 1999     

Mass spectrometry of molecules and radicals in glow discharge plasma

The article represents a method and equipment developed for mass spectrometric analysis of plasma, that is, for measurement of concentration of atoms and molecules, and their fragments, including free radicals. A compact and inexpensive mass spectrometer is based on a quadrupole residual gas analyzer (RGA-200, Stanford Research Systems). The design of the two-section differential pumping chamber makes it possible to bring the mass-spectrometer analyzer to the entrance diaphragm to a distance of 40 mm in order to measure quick reacting and easily condensed particles. The equipment was used for analyzing the composition of spherical glow discharge plasma in methanol vapor and acetone-nitrogen mixture. A procedure for mass spectrum processing is proposed. Time-varying concentrations of all observed neutral particles are measured. Presently available data on sections of complete and dissociative ionization of molecules and their fragments, which are necessary for reconstructing concentrations of particles in plasma from measured mass spectra, are presented.     

Field ion and field desorption mass spectrometry of inorganic compounds

The review on recent developments in field ionization mass spectrometry of inorganic compounds concerns the different mechanisms of ion formation at surfaces and under the influence of extremely high electric fields, field dependent chemical reactivity at surfaces and ion desorption from surfaces for mass spectrometric analysis. Applications in various areas are discussed, where this method has been used to identify surface compounds or to study kinetic phenomena at interfaces.     

Separation of Ammonium and Nitrate for Isotopic Analysis of Nitrogen 15 Using Vacuum Distillation Method

The parameters affecting the vacuum distillation method for quantitative separation of ammonium and nitrate for mass spectrometric determination of ¹⁵N were investigated. The vacuum distillation was found to be advantageous to steam distillation method because no interference from organic compounds was encountered, greater volumes could be processed and no previous evaporation of the water samples was necessary. The mass spectrometric isotopic analysis of nitrogen 15 proved the suitability of the vacuum distillation method for quantitative separation of ammonium and nitrate.     

Sample Preparation for the Determination of Metals in Food Samples Using Spectroanalytical Methods—A Review

Abstract

The present article gives an overview of recent publications and modern techniques of sample preparation for food analysis employing atomic and inorganic mass spectrometric techniques, such as flame atomic absorption spectrometry, chemical vapor generation atomic absorption and atomic fluorescence spectrometry, graphite furnace atomic absorption spectrometry, inductively coupled plasma optical emission spectrometry, and inductively coupled plasma mass spectrometry. Among the most frequently applied sample preparation techniques for food analysis are dry ashing, usually with the addition of an ashing aid, and acid digestion, preferably with the assistance of microwave energy. Slurry preparation, particularly with the assistance of ultrasound, is increasingly used to reduce acid consumption and sample preparation time. Direct analysis of solid samples is gaining importance in the field of food analysis as it offers the highest sensitivity, avoids the use of acids and other aggressive reagents, makes possible the analysis of micro‐samples, and can be applied for fast screening analysis, e.g., of fresh meat.     

电感耦合等离子体质谱法进样技术研究

电感耦合等离子体质谱(ICP-MS)是近年发展起来的新型痕量元素分析技术,可以用于检出限为pg/ml级的痕量元素及天然同位素分析,同位素比分析及常规同位素稀释质谱分析等。所有这些应用都显示出ICP-MS在痕量元素分析领域中具有无与伦比的优点。ICP-MS进样技术一直是人们所关注的     

Detection of small signals in mass spectra

The results of the chromatographic–mass spectrometric analysis of a mixture containing a compound with low protonation efficiency have been given. A software package for preliminary processing of mass spectra is used for determining the peak parameters of the compound ions. The reliability of the processing results has been confirmed by comparison with the tabular data for the isotope masses and the isotopic composition of the component. The mass spectrum has been interpreted by calculating the peak areas and centroids together by evaluating the standard deviation of the center of the peak. The results of processing the mass spectrum using the mMass program have been given.

     

Gas-flow assisted ion transfer for mass spectrometry

Methods and devices that use gas flows to collect ions and transfer them over long distances for mass spectrometric analysis have been developed. Gas flows derived from the ionization source itself or provided by means of additional pumping were used to generate a laminar flow inside cylindrical tube. Hydrodynamic simulations and experimental tests demonstrate that laminar flow can transfer ions over long distance. The typical angular discrimination effects encountered when sampling ions from ambient ionization sources are minimized, and the sampling of relatively large surface areas is demonstrated with desorption electrospray ionization (DESI). Ion transfer over 6 m has been achieved and its application to multiplexed chemical analysis is demonstrated on samples at locations remote from the mass spectrometer.     

Nanoanalysis of the arthropod neuro-toxins

Many kinds of venomous principles modulate physiological responses of mammalian signal transduction systems, on which they act selectively as enhancers, inhibitors or some other kind of effectors. These toxins become useful tools for physiological research. We have employed and characterized paralyzing toxins from the venom of spiders, insects and scorpions with a limited supply. We have developed rapid and sensitive mass spectrometric technology and applied for the identification of these toxins. Venom profiles are screened by MALDI-TOF fingerprinting analysis prior to purification of venomous components, then marked target toxins of small molecular mass (1000–5000) are characterized directly by means of mass spectrometric techniques such as Frit-FAB MS/MS, CID/PSD-TOF MS, Capil.-HPLC/Q-TOF MS/MS etc.     

Structural elucidation of diglycosyl diacylglycerol and monoglycosyl diacylglycerol from Streptococcus pneumoniae by multiple-stage linear ion-trap mass spectrometry with electrospray ionization

The cell wall of the pathogenic bacterium Streptococcus pneumoniae contains glucopyranosyl diacylglycerol (GlcDAG) and galactoglucopyranosyldiacylglycerol (GalGlcDAG). The specific GlcDAG consisting of vaccenic acid substituent at sn-2 was recently identified as another glycolipid antigen family recognized by invariant natural killer T-cells. Here, we describe a linear ion-trap multiple-stage (MS(n) ) mass spectrometric approach towards structural analysis of GalGlcDAG and GlcDAG. Structural information derived from MS(n) (n?=?2, 3) on the [M?+?Li](+) adduct ions desorbed by electrospray ionization affords identification of the fatty acid substituents, assignment of the fatty acyl groups on the glycerol backbone, as well as the location of double bond along the fatty acyl chain. The identification of the fatty acyl groups and determination of their regio-specificity were confirmed by MS(n) (n?=?2, 3) on the [M?+?NH(4) ](+) ions. We establish the structures of GalGlcDAG and GlcDAG isolated from S. pneumoniae, in which the major species consists of a 16:1- or 18:1-fatty acid substituent mainly at sn-2, and the double bond of the fatty acid is located at ω-7 (n-7). More than one isomers were found for each mass in the family. This mass spectrometric approach provides a simple method to achieve structure identification of this important lipid family that would be very difficult to define using the traditional method.     

Validated LC-MS/MS method for quantification of agomelatine in human plasma and its application in a pharmacokinetic study

An analytical method based on liquid-liquid extraction has been developed and validated for analysis of agomelatine in human plasma. Fluoxetine was used as an internal standard for agomelatine. A Betasil C18 (4.0?×?100?mm, 5?μm) column provided chromatographic separation of analytes followed by detection with mass spectrometry. The method involves simple isocratic chromatographic conditions and mass spectrometric detection in the positive ionization mode using an API-4000 system. The proposed method has been validated with linear range of 0.050-8.000?ng/ml for agomelatine. The intra-run and inter-run precision values are within 12.12% and 9.01%, respectively, for agomelatine at the lower limit of quantification level. The overall recovery for agomelatine and fluoxetine was 67.10% and 72.96%, respectively. This validated method was used successfully for analysis of plasma samples from a pharmacokinetic study.     

基于光谱分析的重载车辆变速箱可靠性评估方法研究

润滑油光谱分析是变速箱磨损状态监测的重要手段。以某重载车辆变速箱台架试验中润滑油原子发射光谱分析得到的元素成分含量检测数据为基础,通过相关性分析和磨损机理分析确定了能够反映整机磨损状态和失效特点的金属元素,并对补油、换油后的光谱检测数据进行了修正,将变速箱试验过程中特征金属元素的含量随试验时间的变化规律表示为线性函数的形式。然后,综合考虑检测数据的时序规律与离散性,利用不同时刻光谱检测数据的正态分布均值和标准差进行变速箱可靠性评估,进一步讨论了失效阈值对可靠性评估结果的影响。研究表明,重载车辆变速箱润滑油中的Cu元素浓度与其他金属元素浓度的相关性较高、绝对值较大,既能够反映变速箱整体磨损状态,又便于检测,利用多个试验样本的润滑油Cu元素浓度光谱检测时序数据,可以对重载车辆变速箱进行可靠性评估;若失效阈值取定值,则失效阈值越大,同一时刻变速箱的可靠度越高;若失效阈值取随机分布,则失效阈值的离散度越大,可靠度随时间延长而降低的趋势越缓慢。当可靠度R大于0.9时,失效阈值的均值对可靠性评估结果的影响十分显著,同一时刻变速箱的可靠度随失效阈值标准差的增大而降低。将光谱分析与概率统计学结合进行变速箱可靠性评估方法研究,扩展了光谱分析技术的应用范围,具有创新性。     

靶丸内混合气体的质谱法测量技术

 叙述了四极质谱(QMS)的结构和气体分析质谱(GAM)的定量分析工作原理。四极质谱具有快速扫描响应,较高的响应灵敏度的特点,在经过标准气体校准后,加上独特的气体进样系统,可用于惯性约束聚变(ICF)靶丸内混合气体组分含量及总量的定量分析。同时,在经过坐标尺度放大等手段,可以对混合气体中质量数极为接近的氘(4.028 2)和氦(4.002 6)在高分辨模式下进行基线分离。用四极质谱对各种靶丸结构、不同混合气体种类的气体进行了定量组分分析,为ICF实验用靶提供了同批次实验数据。     

X射线荧光光谱分析经验系数法的理论分析

本文对目前流行的若干经验系数法在理论上进行了推导,导出了一个综合的公式。对目前这些方法中系数的物理意义作了阐述。同时导出了一个按特征荧光相对强度来计算的公式。其公式在实际应用中更为简便。 关键词：     

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介绍了为开展漏孔检测、氘-氦分辨性能及真空检漏技术等相关实验研究而进行的四极质谱计分析与测量系统的研制,描述了真空室结构、抽气设备的选型、测量仪器的选择及控制保护子系统工作方式。对系统进行了包括极限真空、残余气体质谱分析、漏放气率、质谱计性能等测试,结果表明本系统达到了设计要求。     

Reconstruction of the Cadmium Contamination History of a River Floodplain from Maoniuping Mining Area (China) by Gamma Ray Spectrometry and Inductively Coupled Plasma Mass Spectrometry

The Maoniuping rare earth elements deposit is the second largest rare earth elements deposit in China, and the third largest in the world. A sediment core was collected from the river floodplain downstream from the Maoniuping rare earth elements mining area (Sichuan Province, China) to reconstruct the cadmium contamination history and trace its contamination source. Based on lead-210 (²¹⁰Pb) dating by gamma ray spectrometry and elements determination with inductively coupled plasma mass spectrometry of the sediment core, it was found that the cadmium accumulation rate of the flood plain increased from 0.16 to 2.22 µg cm^?2 yr^?1 over the past 100 years. Combining aspects of time, space, and element composition information, it is proved that the exploitation of Maoniuping rare earth elements deposit was the main reason for the increase. Moreover, to evaluate the mobility and availability of cadmium in the sediment core, the modified European Communities Bureau of Reference sequential extraction procedure in combination with inductively coupled plasma mass spectrometry was applied. Risk assessment code was used to further assess the environmental risk of cadmium in the sediment. It was found that the environmental risk from cadmium was high in the surface of the sediments. The results from gamma ray spectrometric and mass spectrometric methods may provide important information for the control and remedy of cadmium-related pollution areas.     

发射光谱分析法测量不确定度的评定与应用

JJF1059-1999<测量不确定度的评定与表示>指出可以用不确定度作为评判分析方法准确度的标准,使得借助标准样品来进行分析的诸多分析方法有望成为标准分析方法.本文对X射线荧光光谱分析和光电直读光谱分析的测量不确定度在铜及铜合金中的评定与应用进行了讨论.     

Model estimated uncertainties in the calibration of a total reflection x‐ray fluorescence spectrometer using single‐element standards

Total reflection x‐ray fluorescence (TXRF) was used for the analysis of single‐element standards, Ca, Cr, Zn, Ga, Se, Rb, Sr and Y, at various concentrations. A triplicate analysis was carried out to determine the homogeneity of the samples and the reproducibility of the results. The average estimated uncertainty (model calculated) values was compared with the predicted uncertainties (systematic or equipment related). The estimated and the predicted uncertainties showed considerable agreement except at very low concentrations resulting from excessive dilution. The discrepancies decreased as the concentrations of the analytes increased. This work indicates a very reliable dependence on the systematic or predicted uncertainties from TXRF spectrometric analysis, especially at high concentrations. Copyright © 2006 John Wiley & Sons, Ltd.     

The interaction of an O2 molecular beam with an Fe(110) surface

The initial interaction between an O₂ molecular beam and a cleaned Fe(110) surface has been studied by a combination of Auger electron spectrometric (AES) and mass spectrometric techniques. The incident molecular beam intensity was calibrated using a stagnation detector, and the initial sticking coefficient for chemisorption was determined by mass spectrometric measurement of the transient in molecular scattering behavior observed when the cleaned surface was exposed to the molecular beam. This permitted an absolute calibration of the AES system for oxygen, and allowed comparison of the kinetic measurements of the oxygen adsorption process by the two techniques. Results indicate that the initial sticking coefficient is 0.2 ± 0.01. Oxygen is initially chemisorbed up to a coverage of 1.6 ± 0.16 × 10¹⁵ cm^?2, by a process following Langmuir kinetics. Beyond this point AES studies indicate a slower rate of oxygen uptake which is independent of gas-phase oxygen pressure. The mass spectrometric studies further indicate that for a cleaned, annealed surface those oxygen molecules which are not chemisorbed are scattered in a non-diffuse manner.